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Epichlorohydrin → 2-Chloro-1-(3-chloro-2-hydroxypropyl)-4-nitroimidazole

HRID 856144
ノート
印刷プレビュー

反応式

HRID 856144 の反応式
C(=O)([O-])O.[Na+].[Cl:6][C:7]1[NH:8][CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[N:11]=1.[CH2:15]([CH:17]1[O:19][CH2:18]1)[Cl:16]>C(#N)C>[Cl:6][C:7]1[N:8]([CH2:18][CH:17]([OH:19])[CH2:15][Cl:16])[CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[N:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7835EpichlorohydrinHCID 516892Sodium BicarbonateHCID 178526855HCID 178526855、化合物

生成物 1

HCID 230812022-Chloro-1-(3-chloro-2-hydroxypropyl)-4-nitroimidazole収率 63%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Sodium hydrogencarbonate (1.25 g, 14.91 mmol) was added to a solution of 2-chloro-4-nitro-1H-imidazole (2 g, 13.56 mmol) and epichlorohydrin (1.38 g, 14.91 mmol) in acetonitrile (60 ml), and the resulting mixture was stirred under reflux for 4 hours. The reaction mixture was allowed to return to room temperature, and concentrated under reduced pressure. To the residue, water (20 ml) was added, the resulting mixture was extracted with methylene chloride (15 ml) twice, and the extracts were dried over sodium sulfate, and then filtrated. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/n-hexane=1/1) to afford 2-chloro-1-(3-chloro-2-hydroxypropyl)-4-nitroimidazole (2.04 g, yield 63%) as a light yellow oil.

後処理

  1. temperatureunder reflux for 4 hours
  2. customto return to room temperature
  3. concentrationconcentrated under reduced pressure
  4. additionTo the residue, water (20 ml) was added
  5. extractionthe resulting mixture was extracted with methylene chloride (15 ml) twice
  6. dry with materialthe extracts were dried over sodium sulfate
  7. filtrationfiltrated
  8. concentrationThe filtrate was concentrated under reduced pressure
  9. customthe residue was purified by silica gel column chromatography (ethyl acetate/n-hexane=1/1)

出典と根拠

ORDレコード
ord-a9fe4db7069540b48be462482aaf123b
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262212B2

反応ノート

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